4. RESULTADOS E DISCUSSÃO
5.0. CONCLUSÕES
As RAMs-BSA estudadas mostraram-se eficiente para a exclusão das proteínas do leite materno, assim como os oligossacarídeos presentes na matriz.
As colunas RAMs com suporte de 3 µm apresentaram eficiência cromatográfica e poderia ser usada no modo simples de eluição proporcionando análises rápidas e sem preparo de amostra. Porém, a forte interação dos analitos com a coluna RAM-BSA causou perdas de eficiência cromatográfica.
Os estudos realizados inferem bons limites de detecção, com todos os parâmetros cromatográficos ajustados, os testes finais na concentração mais alta de trabalho, 100 ng/mL, permitia sensibilidades elevadas ao método.
A metodologia clássica de preparo de amostra, precipitação de proteína, foi avaliada neste trabalho, porém o efeito memória permaneceu mesmo quando foram utilizadas diferentes colunas analíticas, modos de eluição, e o uso de uma matriz substituta (leite bovino), indicando contaminação do sistema cromatográfico, provavelmente no auto-injetor, impossibilitando a validação e aplicação do método desenvolvido.
Existem vários trabalhos analíticos publicados na literatura sobre a determinação das benzofenonas selecionadas em leite materno, a maioria das vezes foi focado na determinação das BPs utilizando técnicas como microextração líquido- líquido dispersiva e extração em fase sólida. O preparo de amostra proposto neste trabalho difere dos reportados na literatura. A injeção direta de amostras utilizando colunas RAMs é considerada uma boa escolha em relação a sua boa capacidade de extração e operação, especialmente quando comparado ao SPE que é tradicionalmente utilizado em análises de fluidos biológicos, porém os analitos de baixa polaridade apresentaram forte interação com as colunas RAMs avaliadas.
A triagem de amostras de leite materno coletadas de 26 diferentes mães da Cidade de São Carlos foi avaliada por LC-HRMS e apresentou a presença de benzofenonas em 88% das amostras analisadas.
Referências
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